CHAPTER 1

INTRODUCTION

1.1 Research Background

Thermoset polymeric porous recently gain high public noticeable due to their
distinct three-dimensional network structure with characteristics of low density, good
mechanical properties, thermal and electric insulation, water treatment, which have been
used in versatile of application such as transport through membranes, chromatography
media, biomedical, electronic, photonics and life science [1][4]. Porous material is a
material which made up of solid matrix either can be rigid or flexible with interconnected
voids [5]. Porous material has been categories into three types which are macro-, meso- and
microporous with pores size greater than 50nm, 50-2nm and less than 2nm respectively [6],
[7]. Conventional porous materials such as zeolites, activated carbon, silicates, metalorganic frameworks, covalent-organic frameworks are generally apply in catalyst support,
adsorbent, gas storage, gas/vapor separation, luminescence and drug delivery [8], [9].
There are numerous methods to fabricate porous polymers such as thermally
induced phase separation (TIPS), chemically induced phase separation (CIPS), gas
foaming, porogen leaching and various templating method [2], [10]. In thermally induced
phase separation method, a polymer solution with suitable solvent is prepared and
undergone quench. After that, the frozen solvent is extracted by freeze drying or vise versa
at high temperature [11]. Chemically induced phase separation produces porous structure by
extraction of the solvent in polymer solution, which is separated after the curing process
[2]. Gas foaming is a method where blowing agent is used to generate porous structure

within the polymer by liberating gas at the same time as the curing of continuous matrix
[12]. Besides, porous structure can be obtained through porogen leaching where porogen is
added before shaping and later being removed [13].
There are a variety of templating method such as colloidal crystal templating,
biotemplating, block copolymer templating and emulsion templating in which, concentrated
emulsion template is the much favorable method because of its simplicity and control of
pore size [10], [14]. The process of emulsion templating is suitable in many kinds of
materials and low cost. It has the advantages of removing the templating phase in the
emulsion system without disturbing the supporting structure. The extraction method can be
easily carried out by evaporation or dissolution [10].
Emulsion is a colloidal dispersion of two liquids that are incapable for being mixed
(immiscible liquids). It is also being described as a system that consists of one liquid is
dispersed throughout another one which is the continuous phase [15]. In most cases, one of
the liquid in the emulsion is water while the other is resin as the oil phase. In single
emulsion, depending on the ratio of oil to water, emulsion can be oil-in-water (O/W) system
or water-in-oil (W/O) system. Oil-in-water (O/W) emulsion is made up of oil droplets
dispersing in aqueous phase whereas water-in-oil (W/O) emulsion is made up of water
droplets dispersing in oil phase. Emulsion is formed by applying energy through agitating
into the liquid mixture so that to overcome the interfacial tension [16]. The process to
produce emulsion is known as homogenization. Homogenizer is generally used during
homogenization process, in which high mechanical agitation is applied to the liquids by
using homogenizer; and therefore emulsion system can be formed [17].
Emulsion stability is crucial to maintain their properties as long as possible.
Emulsion is thermodynamically and the destabilization of emulsion are usually occurs
through flocculation, coalescence, and finally phase separation or sedimentation [16].
Firstly, the flocculation of droplets in emulsions involves aggregation to form clusters.
Then, due to the rupture of interface film between the droplets, the flocculation will
undergo coalescence and fuse to form larger droplets. Finally, it can eventually cause major
phase separation or sedimentation under the influence of gravity. The stability of emulsion
depends primarily on a rigid protective film encapsulating the droplets present in the
2

emulsion system [18]. The distribution of the droplets size is strongly related to the stability
of the emulsion system. Therefore, normally emulsifier which are surface-active molecules
is added to stabilize the emulsion system by acting as a bridge between water and oil
interface so that surface tension can be reduced thus prevents the flocculation of droplets
[16], [19]. Consequently, it provides emulsion kinetic stability by preventing contact
between the two or more droplets, coalescence and macroscopic phase separation [20].
Diglycidyl ether of bisphenol A (DGEBA) epoxy resin is selected to used in this
research because it exhibits superior properties such as mechanical strength, excellent
adhesion, high chemical and corrosion resistance, high heat resistance, dimensional stability
properties and durability in harsh environment [21]. Besides, versamide-polyamide is used
as a curing agent due to its emulsifying ability and other advantages of little volatility and
toxicity, good compatibility with resin and no strict requirement of chemometrics [4], [22].
This study describes the emulsion system changes from oil-in-water (O/W)
emulsion to water-in-oil (W/O) emulsion by controlling the epoxy/water volume ratio.
Hence, the microstructure of the emulsion also experienced the changes in the type of
disperse phase and continuous phase. When the volume ratio of the minor components
increases up to the percolation point it will lead to phase inversion. Now, the previous
dispersing phase becomes the continuous phase. Further curing of epoxy and polyamide
hardener is expected to solidify the epoxy phase in the emulsion. From there, epoxy microparticles and epoxy porous are expected to fabricate. Water can work as the void-template
of epoxy porous in the water-in-oil (W/O) system to produce epoxy porous. Higher porosity
could be prepared from solidifying the flocculating epoxy droplets in water or partly
coalescence so that these epoxy particles can adhere each other to form micro-sphere
packing porous. The structure of porous epoxy exhibits fully interconnected pores and is
made up from the packing of micro and sub-micro epoxy particles [23].
1.2 Problem Statements
Porous material can be prepared by thermally and chemically induced phase
separation, gas foaming, porogen leaching [2], colloidal crystal templating, biotemplating,
emulsion droplets templating and sol-gel techniques [10]. All those method producing
porous material involve the use of solvent or porogen to form porous structure. These
3

solvent used will cause environmental issues and should be avoided. The use of blowing
agent to fabricate foam will be cost. In addition, foaming process is also difficult to control
because of the increase in viscosity via the curing process. In this research, aqueous
emulsion method is used to prepare porous epoxy. This method is simple, low cost and
greener approach as it only uses water as void template instead of solvent and no emulsion
of volatile products, as well as no usage of blowing agent [4], [24].
The stability of emulsions are affected by various aspect such as epoxy/water
volume ratio, epoxy/polyamide volume ratio and homogenization condition. The phase
volume ratio consequently influences the viscosity of emulsion and droplet size produced.
In addition, the droplets sizes formed during homogenization determine the emulsion
stability and microstructure of the porous epoxy. The interfacial area will increase due to
the reduction is the size of droplets and this can cause coalescence [17]. The water droplets
dispersed in the oil continuous phase has high mobility that can easily lead to emulsion
instability such as flocculation and coalescence [25]. Therefore, the epoxy/water ratio and
epoxy/polyamide ratio required to be aware on production on porous epoxy since it alters
the properties of the porous epoxy produced.

1.3 Objectives
The research is focus on O/W and W/O aqueous emulsion in preparation of epoxy
particles and porous epoxy. Main objectives of this research are:
i. To study the effect of epoxy/water ratio on viscosity of aqueous epoxy emulsion and
morphology of epoxy phase after curing.
ii. To study the effect of epoxy/polyamide ratio on viscosity of aqueous epoxy
emulsion and morphology of the obtained porous epoxy.

1.4 Scope of Study

The scope of this research is to prepare epoxy particles and porous epoxy using
aqueous emulsion to investigate the morphology and mechanical properties by different
emulsion formula. Epoxy particles and porous epoxy is prepared by controlling the
epoxy/water volume ratio from 0, 0.1, 0.2, and 0.3 continuously up to 1. The microstructure
of the epoxy emulsion prepared is observed under the optical microscope (OM). The
procedure is carried out to study the changes of microstructure in epoxy emulsion from oilin-water (O/W) to water-in-oil (W/O) emulsion in order to investigate the volume fraction
of epoxy needed to prepared co-continuous phase which porous epoxy can be produced.
Viscosity of the epoxy emulsion is examined using Brookfield viscometer and gel time is
investigated by using probe method. After that, the epoxy emulsion undergoes curing and
post-cured process. The obtained epoxy particles or porous epoxy is undergone morphology
characterization and mechanical testing. The morphology of epoxy particles and porous
epoxy is analyzed under Scanning Electron microscope (SEM) and Optical microscope
(OM) to determine the effect of emulsion formula on the morphology of epoxy particles
and porous epoxy. The physical properties such as density and porosity are investigated by
helium pycnometer and BrunauerEmmettTeller (BET). Compression is measured using
an Instron machine to evaluate the mechanical properties of porous epoxy with various
emulsion formula.
CHAPTER 2
LITERATURE REVIEW

2.1 Emulsions
Emulsions system are consists of two immiscible liquids where one liquid is
dispersed within the another type liquid in the form of fine droplets. The two most basic
type of emulsion are oil-in-water (O/W) and water-in-oil (W/O) emulsion. The composition
of continuous and dispersed phase determine the type of emulsion which forms [26]. The
5

emulsions are usually prepared by apply very high rates of mechanical agitation to the
liquid include high-speed stirrers, microfluidic devices, ultrasonic homogenizer, highpressure homogenizers, and mechanical homogenizer. This vigorous agitation generate high
shear force when preparing emulsions and result in reduction of droplet diameter [17].
The emulsions system are thermodynamically not stable because of the interfacial
free energy [27]. The interfacial free energy arises due to the attractive forces present
between two same characteristic molecules (cohesive force) such as water-water and oil-oil
is higher than of the attractive forces present between two different characteristic molecules
(adhesive force) such as water-oil [28]. Therefore, after some time, the emulsions will more
favorable to form phase separation [29].
Generally, emulsifiers is added to reduce interfacial tension by absorbed onto the
surface of the droplets and thereby shield and inhibit the flocculation of droplets [17].
Besides, the emulsifiers also promote the increase in adhesive force between oil and water
thus stabilize the interfacial film and as a result stabilize the emulsion [30]. Emulsifier has
lipohilic tail and hydrophilic head that can react with oil and also water. These interactions
can stabilize the emulsion by reduce the surface tension and forming barrier around the of
the dispersed droplets. There are many types emulsifier with different functionalities that
determine the formation of the barrier includes electrostatic repulsion, creation of a bound
water layer, and steric hindrance [31].

2.1.1

Types of Emulsion

There are two basic classification of emulsion which are oil-in-water (O/W) and
water-in-oil (W/O) emulsion [31]. O/W emulsion is formed when oil droplets are dispersed
throughout the aqueous continuous phase while W/O emulsions is vice versa [32]. In
addition, there are also multiple or double emulsion which are water-in-oil-in-water
(W/O/W) and oil-in-water-in-oil (O/W/O). Double emulsions are complex emulsion system
whereby the dispersion of droplets in liquid (O/W or W/O emulsion) are further dispersed
throughout another liquid phase. The internal dispersed droplet are separated from the

external continuous phase by a layer of another phase [33]. All these type of emulsion are
illustrated in Figure 2.1 [34].

2.1.1.1

Figure 2.1: Type of emulsions [34].

Oil in Water Emulsion (O/W)

Oil-in-water emulsion system consists of oil droplets dispersed within the aqueous
phase where oil is the internal or dispersed phase while the aqueous solution is external or
continuous phase. This type of emulsion usually formed when the aqueous phase contribute
more than 45% of the total weight and a hydrophilic (water loving) emulsifier is applied
[35]. The immiscibility of oil and water urge the use of emulsifier to stabilize emulsion.
Different type of emulsifier have specific HLB (hydrophile-lipophile balance) value that
stabilize different type of emulsions. Emulsifier with HLB (hydrophile-lipophile balance)
value 8-18 are more hydrophilic and suitable for oil-in-water emulsion [36].

2.1.1.2

Water in Oil Emulsion (W/O)

Water-in-oil emulsion is comprised of water droplets dispersed within the oil phase
where water is the internal or dispersed phase while oil is external or continuous phase.
W/O emulsion usually formed when the aqueous phase contribute less than 45% of the total
weight and a lipophilic (oil loving) emulsifier is applied [35]. Common method to stabilize
7

the emulsion system is by using emulsifier or surfactant. Emulsifier has a crucial roles to
reduce the surface tension as to promote formation of emulsion. Emulsifier with HLB
(hydrophile-lipophile balance) value 3-6 are more lipo loving and suitable for water-in-oil
(W/O) emulsion [36].
The stability of water-in-oil (W/O) emulsion can be classified into stable emulsions,
mesostable emulsions and unstable emulsions. The changes of emulsion properties is varied
according to the stability of emulsion. These classification of water-in-oil (W/O) emulsion
stability can be differentiate by lifetime, physical appearance and rheology properties. The
viscosity of stable emulsions increase at least three times than the initial viscosity over
time. Unstable emulsion undergoes phase separation after emulsification within few hours.
In some of the case where the oil phase are highly viscous then the water may be retained.
Mesostable emulsion has the intermediate properties of stable and unstable emulsion. There
might be possible for the water droplets remain stable for some period of time in the
condition of oil viscosity is sufficiently high [37].

2.1.1.3

Effect of Volume Fraction on Emulsion Type and Viscosity of Emulsion

Figure 2.2 shows the effect of volume fraction of oil on the emulsion viscosity.
Epoxy and water is an immiscible system. The morphology of the emulsion is controlled by
the relative volume fraction of two components. When epoxy are mixed with water, phase
separation occur where epoxy is separate from the water into little spherical globs (isolated
phase). Oil is the major component while water is the minor component. At the beginning,
the aqueous liquid epoxy resin is disperse in water which is known as oil-in-water (O/W)
emulsions and it is liquid-liquid dispersion system. When curing is occur at this stage, the
liquid epoxy started to crosslink and it become solid-liquid dispersion system and it will
produce epoxy resin particles. The viscosity of emulsion show increment as the volume
fraction of oil increases until a critical point. The viscosity of emulsion increase due to
epoxy has higher viscosity than water. Besides, when the fraction of oil increases, it would
lead to coalescence of oil droplets and the development of a coarser morphology. Now,
8

there is no more isolated phase but is in bicontinuous phase. At this critical point, the
emulsion viscosity tend to drop and this signifies inversion of phase. If keep adding the
volume fraction of oil, the oil will become the major component and water is the minor
component. The water will become isolated phase and surrounded by continuous phase of
epoxy. Start from the inversion zone, as the crosslink reaction happen, it can produce a
porous epoxy.

Figure 2.2: The influence of volume fraction on the emulsion type and viscosity of a
typical emulsion [15].

2.1.2

Emulsion Stability

Emulsion stability is defined as the capability to resist changes in its properties

throughout time. The more stable is the emulsion, the properties of the system will
undergoes changes in a slower rate [17].

Stable emulsion are characterized by low

interfacial tension, high surface viscosity, strong steric repulsion, small density difference
between phases, small droplet size and so on [15]. Therefore few factors that affect the
emulsion stability and it is important to determine the rate of coalescence and consequently
break down of emulsion system. The factors to determine emulsion stability are interfacial
9

film physical nature, electrical or steric barrier, continuous phase viscosity, droplet size
distribution and temperature [38].

2.1.2.1 Interfacial Film Physical Nature

Collision between the liquid dispersed droplets in the emulsion system are
frequently happen due to their constant Brownian movement. Therefore, the breaking of
interfacial film encapsulate the colliding droplets at the point of contact cause them
coalesce and form a larger droplet [38]. The total free energy of the emulsion system is
reduced when the droplet size is increased which indicate the instability of the emulsion
[39]. If this process keep going on, it will cause phase separation in the emulsion system.
As a conclude that the interfacial film strength is crucial in maintain the stability of
emulsion. The stronger the strength of the interfacial film, the more stable is the emulsion
system. The strength of this interfacial film is depend on the structure and spatial
arrangement of atom in the emulsifier used [40].

2.1.2.2 Droplet Size Distribution

Droplet size distribution can be classified into two types which include
monodisperse and polydisperse. Monodisperse is characterized by uniform droplet size
where all the droplets has almost the similar diameter size. In contrast, polydisperse has
non-uniform size of droplets and a range of droplet size. The size of droplets distribution
affect the coalescence rate and consequently emulsion stability. The droplet size distribution
are affected by operating parameter and the properties of the liquid such that speed of
agitation, difference in viscosity between two phase and also type of emulsifier. Large
droplet and broad size of distribution have higher tendency to cream and coalesce compared
to smaller droplet and narrow distribution size [41]. Higher mechanical agitation into the
liquids produce smaller droplets and narrow size distribution. The droplets size distribution

10

are related to the interfacial area. As the diameter of the droplets become smaller, the
interfacial area will increase [38].

2.1.3

Temperature

Temperature of emulsion is crucial in affecting the emulsion stability. The stability

of emulsion changes as the temperature changes. As the temperature increase, the mobility
of the droplets also increase due to increase in kinetic energy gained. Therefore, the dropletdroplet collision frequency is higher. In addition, the collision between the droplets become
more vigorous with additional average kinetic energy thus it can rupture the interfacial film
surround the dispersed droplets and promote the flocculation and coalescence to occur. The
change in the temperature will also cause the change in the solubility of the emulsifier. The
emulsifier show the most effective of its function when near to the point of minimum
solubility in the solvent [38]. Other than that, high temperature also affect the
conformational changes in emulsifier molecules which in turn affect their ability of
stabilization [42].

2.1.4

Emulsion Instability

Emulsion is thermodynamically unstable in which they tend to undergoes phase

separation. The emulsion system can retain stability when there is the strong electronic
repulsion between the dispersed droplets and has high strength of interfacial film [43].
When the stability of emulsion is diminished, it will slowly undergoes breakdown and
phase separation is happen. There are several type of breakdown process such as creaming,
sedimentation, flocculation, coalescence and Ostwald ripening as illustrated in the Figure
2.3 [44].

11

Figure 2.3: The breakdown processes of an unstable emulsion [44].

Creaming and sedimentation process are arises from gravity forces and large
difference in specific gravity between dispersed phase and continuous phase. The phase
that has lower density will rise to the top and form the cream while the phase that has
higher density will occupy the bottom layer [44]. The droplets size still remain the same
as the droplets are still encapsulated by the interfacial film [45].

In the emulsion system, the individual dispersed droplets are usually in constant
Brownian movement [45]. So, collision between the droplets is to be unavoidable. The
frequency of collisions are also being affected by factors include thermal energy and
gravitational force. When collision take place, the dispersed droplets are either remain
distance from each other or floc depend on the magnitude of attraction force and
repulsive force that exists in between the droplets [46]. Flocculation occurs when the
attraction force is overwhelmed the repulsive force. During this process, the individual

12

droplets remain their integrity and retain the size of droplets. As more and more
droplets are come together, three-dimensional clusters will be formed [45].

Moreover, Ostwald ripening is also one the process that indicate unstable
emulsion system which results from the limitation solubility in the continuous phase.
This can be seen in the growth of dispersed droplets due to smaller droplets has high
solubility that cause transportation of molecules through the continuous phase . This
kind of breakdown of emulsion happen even the droplets are not touched each other's
[44], [45]. Finally, the combination of two or more droplets to form a single larger
droplets which referred as coalescence. In this process, the interfacial film is broken
during collision and consequently the droplets fuse together [34]. If this process is
continues, phase separation of emulsion will occurs. Besides, phase inversion occurs
where the dispersed phase become continuous phase and vise versa.

2.2

Homogenization
Homogenization is a process whereby mechanical stress is applied to two

immiscible liquids so that dispersed phase can be physically break down into small droplets
therefore emulsion is formed [47]. It is widely used to produce emulsion where the
interfacial tension between the continuous phase and disperse phase is being deformed by
mechanical agitation [48]. There are two type of homogenization which are primary and
secondary homogenization. Primary homogenization is refer as formation of emulsion
directly from two liquid that are incapable of mixing while secondary homogenization
reduced the droplets size in an currently existing emulsion [49]. Since secondary
homogenization has been undergoes homogenization process for twice therefore it has
smaller emulsion droplets than primary homogenization [46].
There are many type of homogenizer is developed for different purpose such as high
speed homogenizer, high pressure valve homogenizer, ultrasonic homogenizer [47], high
13

pressure jet homogenizer [50], edge-tone resonant homogenizer and etc [48]. Generally, the
commercial homogenizer comprised of small blade that driven by the motor at the end of
the rotor shaft. The rotating small blade within the rotor shaft create high shear rate which is
a strong disruptive shear forces that lead to formation of small droplets in the emulsion
[51].
Rotor-stator homogenizers which also known as high speed homogenizer are
commonly used to produce liquid-liquid emulsions through the formation of droplets by
mixing two immiscible liquids at very high speed and high shear rate. In agitated liquidliquid systems, there consist of two opposite processes occurs in emulsification process
which are break up of droplets and coalescence. Smaller droplets is formed from the
breakup of large droplet but latter it formed larger droplets from two or more smaller
droplets [52]. Since the homogenization has short process cycle, cost reasonable and it can
be used for high volume production. Thus, high speed stirring by rotor-stator homogenizer
is very practical in producing of nanoemulsions as well as macro-emulsions [53].
Rotorstator homogenizers is featured by a small gap between the rotor and the
stator with a high rotor tip speed, which generates very high shear rates in the gap and very
high energy dissipation rates in the stator region [52]. The shearing rates is depend on the
rotor tip speed. Thus, the size of disperse droplets is reduced by a combination of extreme
turbulence, cavitation and mechanical shearing occurring within the narrow gap between
the rotor and the stator [51]. When the rotor tips is rotate at very high speed, the shearing
action will cause the generation of heat which will affect the emulsion stability [54]. The
rotor-stator principle of the IKA Ultra-Turrax

T 25 Digital is shown in Figure 2.4 and

Figure 2.5 [55].

Figure 2.4: Dispersion principle in rotor-stator homogenizer [55].

14

Figure 2.5: The cross section of rotor-stator head of homogenizer [51].

2.3

Thermoset - Epoxy

2.3.1

Epoxy Resin
Epoxy are polymers that are classified as thermoset which are widely used in

versatile of applications such as adhesives, automobile, flooring, structural materials,

printed circuit board (PCB) and so on [56]. It exhibited superior properties such as low
shrinkage upon cure, good mechanical strength, excellent adhesion to a variety of substrate,
high

chemical and corrosion resistance, high heat resistance, dimensional stability

properties and durability in harsh environment [21]. The properties of epoxy resin is depend
on the its chemical structure, type of hardener used, filler content and also cross-link
density [57].
Epoxy resins are low molar mass prepolymer which comprised of at least two
epoxide group in its molecular structure [58], [59]. Most of the cured epoxy resin are
prepared from epoxy prepolymer with curing agent. There are various epoxy resin available
which are bisphenol A epoxy resin, cresol novolac, phenol novolac, glycidyl ether, Peracid
resins, Hydantoin, cycloaliphatic, glycidyl amine, heterocyclic epoxy and so on [60].
Diglycidyl ether of bisphenol A is the most common epoxy that use along with
epichlorohydrin in the presence of base catalyst for preparation epoxy thermoset which
occupy 75% in worldwide industrial application [61]. Epoxy thermoset can be produced via
15

condensation polymerization between bisphenol A and epichlorohydrin as illustrated in

Figure 2.6.

Where n=0.25

Figure 2.6: Chemical structure of diglycidyl ether of bisphenol A (DGEBA) epoxy resin
[62].
The epoxide functional group in the epoxy resin are responsible for crosslinking
reaction. Active hydrogen (H active) from any curing agents such as amines, amide, acids
and anhydrides can easily react with the epoxide group due to high reactivity of epoxide
group. The curing reaction can take place at room temperature if high reactive amine is
used [63].
Many researches had been done by using DGEBA epoxy resin as polymer matrix in
various type of fields. For instance, Dai. C et al. had synthesize the three dimensional (3-D)
porous epoxy by reactive encapsulation of suitable solvent via crosslinking reaction of bifunctionality diglycidylether bisphenol-A (DGEBA) and triphenylolmethane triglycidyl
ether (TGTPM) with polyethylene glycol (PEG). In this research, they also reported
research showed decrement in dielectric constant by introducing porous structure in
thermoset matrix [64].
2.3.2 Curing Agent/Hardener - Polyamide
Polyamides used in curing of epoxy resins is reactive as its structure has many
active site for reaction such that primary amine, secondary amine and reactive amide
(Figure 2.7). It has a relatively high amine value and has a lower molecular weight and
viscosity. It is supplied in solid form with maximum high formulation flexibility. Besides, it
has the advantages of good chemical resistance against water, alkali solutions, alcohols and
16

moderate to poor against acids and solvents [65]. Moreover, polyamide has the
characteristic of emulsifiability. The polyamide which is polar group tend to form physical
bond with polar water as shown in Figure 2.8. Therefore, it prevent the polyamide come to
each other and cause the increase in mobility. The applications for polyamide includes
adhesives, sealants, putties, cable jointing, concrete repair compounds and surface coatings
[65].

Figure 2.7: Structures of dimer acids and polyamide Versamids [66].

17

Figure 2.8: Interaction between polyamide and water [4].

During the crosslink reaction between the epoxy group and the active amine
hydrogen in the structure of polyamide, the epoxy ring is initially opened and OH group is
formed by bond hydrogen provided by amine. At the same time, the amine molecules
formed bond with CH2 group [67]. The primary amines in the polyamide structure is more
reactive than polyamide due to there is less steric effect. The primary amine reaction with
epoxy group is shown in the Figure 2.9. The primary amine is able to react with epoxy
group to form secondary amine. After that the secondary amine will undergoes further
reaction. As the reaction proceed, it will result in three dimensional network which is
illustrated as Figure 2.10.

18

Figure 2.9: Reaction between epoxy group and amine group in polyamide [68].

19

Figure 2.10: Schematic diagram of the network structure formed from the reactive between
DGEBA and diamine hardener [67].

Furthermore, polyamide structure also consists of amide group which is CONHgroup. The crosslink reaction is initiated by the ring opening of epoxy resin and formed
OH-group with active amide hydrogen. Then, the amide group is bonded to the CH 2- in
epoxy resin. The reaction of between epoxy and polyamide is illustrated as Figure 2.11
below [69]. As reaction keep going on, a network structure will formed.

20

Figure 2.11: Reaction between epoxy resin and polyamide resin [69].

2.3.3

Rheology of Epoxy
Polymer rheology is the science of deformation and flow behavior under controlled

condition of polymer [70], [71]. Rheology involves the measurement of viscosity and the
study of polymer flow [72]. Viscosity is the most crucial properties of rheology which
indicated as the resistance to flow [73]. It is important for polymer processing to tailor and
control the process so that optimum polymer properties can be obtained. Epoxy are
generally produced as liquids form at various viscosity and undergoes further
polymerization to complete crosslinking reactions. At the final stage, the epoxy will solidify
in three dimensional crosslink in desired shape. Figure 2.12 shows the viscosity of curing
epoxy [74]. Upon temperature increase, the viscosity is decrease at the beginning due to
polymer is non-Newtonian material. Then, the viscosity of epoxy increase as curing
reaction take place. The viscosity show increment as the curing reaction proceed until it is
fully crosslink and harden. After the epoxy is solidify, there will be no more viscosity.
21

Figure 2.12: Viscosity of curing epoxy [74].

One of the factors that affect the viscosity of curing epoxy is due to the structural
development in epoxy as shown in Figure 2.13. At the beginning (stage A), it consist of
unreacted monomers and curing agents whereby the resin is still fusible and soluble. The
resin are now in low viscosity. Then, stage B indicated the formation of small branched of
molecules as cure begins and monomers start to react with curing agents. In stage B, the
small branches still have degree of freedom to flow. As the curing reaction continue proceed
to stage C, the molecular weight of the resin increase due to formation of longer chain in
the resin and this lead to an increase in viscosity. In stage C, the resin reached gel point
where the viscous liquid is converted to an elastic gel. The final stage D show fully three
dimensional crosslinking at which the molecular weight of the resin increase to infinity. The
resin is now become hard, infusible and insoluble [75].

22

Figure 2.13: Structural development in thermoset during curing process [75].

2.4

Porous Medium

2.4.1

General Concept of Porous Medium

Porous medium is also known as cellular material that containing pores in solid

matrix and has 0.2-0.95 porosity [76], [77]. Porous polymers is a material that give rise to
high porosities and large surface area [78]. The high porosity is benefit in permeability but
it lower the mechanical properties of material while large surface area is used in catalysis
application. Porous material is being categorized based on pores size and pores shape [76].
Porous material have two type of pores dispersed within the medium which are
effective pores (interconnected pores) and isolated (non-interconnected) pores. Different
23

kind of microscopic structure of the porous media give rise to different properties [79].
There is also a various pores shape include open pores, closed pores, through pores and
blind pores as expressed in Figure 2.14 [80]. Closed pores is an isolated cavities within the
material while open pores is the cavities that can contact to the outer surface. Through pores
is the one that connect to outer of another surface of material whereas blind pores cannot
[81]. Different type of pores shape exits within the porous media will result in different type
of pores size [77]. Porous material can be categories into three type which are macro-,
meso-and microporous with pores size larger than 50nm,50-2nm and less than 2nm
respectively [6], [7]. Porosity is expressed as total volume fraction of void space to the solid
occupied volume and it is calculated from relative density and bulk density as below [82].
Total Porosity=1-

bulk density
relative density

(2.1)
Accessibility
a: Close pores
b, c, d, e, f: Open pores
b, f: Blind pores
e: Through pores

Shape
c: Cylindrical open
f: Cylindrical blind
b: Ink-bottle shaped
d: Funnel shaped
g: Roughness

Figure 2.14: Various type of pores shape [77].

2.4.2

Fabrication Methods of Porous Medium

Generally, the thermoset-based porous material is fabricated using chemically

induced phase separation (CIPS) or named as polymerization induced phase separation

(PIPS) method. This method is done through cross-linking polymerization reaction that
encapsulate suitable solvent [64]. Through curing process, phase separation occur where

24

one is polymer-rich continuous phase and the other is solvent-rich droplet phase. The
porous structure is formed after the extraction of the solvent-rich droplet phase [2].
Thermally induced phase separation can used to generated porous structure of
thermoplastic or thermoset-based polymer. This method is temperature-dependent solubility
of polymers. In producing thermoplastic-based porous material, the decreasing in
temperature will lead to decrease in polymer solubility and hence phase separation occurs.
On the other hand, thermoset-based porous material experience decrease in polymer
solubility at high temperature and therefore induced phase separation [83].
Others method includes porogen leaching, gas foaming and fused deposition
modeling. Porogen leaching is a process in which porous structures is generated by adding
porogen into the molten polymer and remove it afterwards. Gas foaming method is by
introducing high pressure carbon dioxide into the polymer as the blowing agent [84].
Besides, fused deposition modeling (FDM) method can be used to produce porous material
such as scaffolds for tissue engineering application. It is work by using a rapid prototyping
technology [85].

2.4.3

Type and Properties of Porous Medium

Porous materials are present everywhere. For instance, bones, soil, rock, sand filters

for water purifier, root zone in agriculture, zeolites, activated carbon and so on [86]. Porous
materials have different type porosity which categorized into low porosity, middle porosity
and high porosity. Low and middle porosity of porous materials usually have closed pores
while high porosity materials are classified into honeycomb materials, lotus-type porous
materials, three dimensional reticulated foamed materials and bubblelike foamed material
[87]. There are four type of porous structure such as dots (0D cavity), channels (1D space),
layers (2D space) and intersecting channels (3D space) shown in Figure 2.15.

Dots (0D cavity)

25

Channels (1D space)

Layers (2D cavity)

Intersecting Channels (3D space)
Figure 2.15: Type of porous structure [88].
The porous material has many important characteristics includes biological,
mechanical and permeability and other properties. In biological aspect, porous structure has
the advantages of light weight and high specific surface area which makes it
biocompatibility. Moreover, the porous material has higher impact toughness. The pore
structure also give rise to good permeability as it is related to the porosity and pore size of
the materials [89]. In addition, the porous material also heat transfer ability, energy
absorption, sound insulation and good damping properties [90].

CHAPTER 3
METHODOLOGY

3.1 Materials
3.1.1

Epoxy Resin
D.E.R 331 epoxy resin is a general purpose, widely used clear liquid resin is

obtained from DOW Chemical Company. The properties of D.E.R. 331 epoxy resin are
shown in Table 3.1 [91].
Table 3.1: Properties of D.E.R 331 epoxy resin [91].
26

Properties
Epoxide Equivalent Weight (g/eq)
Epoxide Percentage (%)
Epoxide Group Content (mmol/kg)
Color (Platinum Cobalt)
Viscosity @ 25C (mPas)
Hydrolyzable Chloride Content (ppm)
Water Content (ppm)
Density @ 25C (g/ml)
Epichlorohydrin Content (ppm)
Shelf Life (Months)
3.1.2 Polyamide

Value
182 - 192
22.4 - 23.6
5200 - 5500
75 Max.
11000 - 14000
500 Max.
700 Max.
1.16
5 Max.
24

Polyamide A062 is an amber liquid and standard medium-viscosity polyamide is

obtained from DOW Chemical Company. The properties of polyamide A062 are shown in
Table 3.2 [65].
Table 3.2: Properties of epoxy curing agent polyamide A062 [65].
Properties
Appearance
Color (Gardner)
Viscosity @ 25C (mPas)
Amine Value (mg KOH/g)
Specific Gravity @ 25C
Flash Point
Equivalent weight per H active
Recommended Use Level phr (EEW=190)
Typical Handling Properties
Gel Time (150g @ 25C), minutes
Thin Film Set Time25C (hours)
Typical Cure Schedule

Value
Amber Liquid
10 Max.
35 - 45
330 - 360
0.96
200
110
60
200
10
(i) 2-7 days at room temperature
(ii) 2 hours @ 60C + 1 hour at 100C

Typical Performance
Following cure schedule (ii)
Heat distortion temperature, C
Flexural Strength, N/mm2

3.1.3

62
86

Distilled Water

27

Distilled water is obtained from water distillation machine (Favorit W4L). The
distillation process is a simple evaporation-condensation system in which the tap water is
boiled to form steam. After the steam undergoes condensation then it is being transfer to
container that are free of contamination. Finally, the distilled water was collected while the
impurities are left behind in the boiling. Distilled water collected is free from impurities
where impurities can affect the emulsion stability.

3.2 Preparation of Epoxy Particles/Porous Epoxy

The recipes of all reagents used to produce epoxy emulsion were shown in Table
3.3. Epoxy and polyamide were pre-mixed homogeneously using an overhead stirrer at 300
rpm for 3 minutes. After that, the epoxy mixture was added into distilled water and stirrer
for 2 minutes at 1000 rpm at room temperature, and then and emulsified using an ULTRATURRAX homogenizer (IKA) at the speed of 5,000 rpm for 2 minutes at 80C water bath.
The epoxy emulsion was then casted into a polypropylene (PP) mould. Emulsion
sample for morphology was picked up and observed using optical microscope. Then, the
casted emulsion was allowed to cure at 80C for 24 hours and post cure at 110C for 2
hours in an oven. This is to remove all the distilled water. The process of preparing the
epoxy emulsion was repeated with different emulsion formula. In this study, the
epoxy/water volume ratio and epoxy/polyamide volume ratio were manipulated to
investigate the effect its effect towards the production of porous epoxy.

Table 3.3 Formulation of epoxy emulsion.

No. Epoxy/Water Epoxy/Polyamide

1
2
3
4

Epoxy

Polyamide

Epoxy

Distilled

Ratio

Ratio

(g)

(g)

mixture

water (ml)

0E:10W
1E:9W
2E:8W
3E:7W

10E:6PA
10E:6PA
10E:6PA
10E:6PA

0
20.175
40.350
60.525

0
12.105
24.210
36.315

(ml)
0
30
60
90

300
270
240
210

28

5
6
7
8
9
10
11
12
13
14
15

4E:6W
5E:5W
6E:4W
7E:3W
8E:2W
9E:1W
10E:0W
EP4E:6W
EP7E:3W
EP4E:6W
EP7E:3W

10E:6PA
10E:6PA
10E:6PA
10E:6PA
10E:6PA
10E:6PA
10E:6PA
10E:10PA
10E:10PA
10E:20PA
10E:20PA

80.700
100.875
121.050
141.225
161.400
181.575
201.750
63.060
110.355
40.76
71.33

48.420
60.525
72.630
84.735
96.840
108.945
121.050
63.060
110.355
81.52
142.66

120
150
180
210
240
270
300
120
210
120
210

180
150
120
90
60
30
0
180
90
180
90

3.3 Epoxy Particles/Porous Epoxy Characterization and Testing

3.3.1

Epoxy Emulsion

3.3.1.1

Emulsion Viscosity

The apparent viscosity of the emulsion is determined by using RVT 230 Brookfield
(Brookfield Eng. Lab., Middleboro, MA, USA) under ambient temperature. Viscosity is
interaction forces of molecules that affect the flow properties of emulsion which involve the
two-phase flows between water and oil phase [92], [93]. The viscosity was determined by
means of Brookfield viscometer which measures the torque produced on a specific spindle
driven by an electric motor to rotate at a constant rotational frequency and at a controlled
rate of shear while immersed to a specified depth in the epoxy emulsion [94].
The epoxy emulsion was prepared by homogenized the epoxy mixtures with
distilled water in a 500ml beaker in 80C water bath. The viscosity for different epoxy
emulsion formulation was recorded respectively. The measurement was made on the epoxy
emulsion using spindle number 3 and rotational speed of 10 according to ASTM D 2196.
The apparent viscosity was obtained by multiplying the torque reading by a coefficient
which depends on the rotational frequency and size of the spindle.

3.3.1.2

Gel Time

29

The gel time of epoxy emulsion were determined by probe method according to
ASTM D 3532 in an isothermal condition that is 80C. The epoxy emulsion was prepared
and casted into a 300ml Polypropylene (PP) mold. Then, the stopwatch was started when
the epoxy emulsion was placed in 80C.
At interval, emulsion surface was probed with wooden stick. At the point at which
the viscosity of epoxy emulsion increase and strings cannot be formed by contact with the
wooden stick, the stopwatch was stopped and the gel time was recorded. Gel time is the
elapsed time where a semi solid gel was formed.

3.3.1.3

Morphology

The microstructure of epoxy emulsions were visualized using a Dino-Lite digital

microscope (AM5216ZT) at different magnification. The background of the images were
adjusted for a white balance and filtered for noise. Photographs of the images were taken
using Dinocapture 2.0 software. Image J was used to measure the mean droplets diameters
with more than 100 droplets were included.

3.3.2

Epoxy Particles and Porous Epoxy

3.3.2.1 Surface area and porosity

BrunauerEmmettTeller (BET) model Micromeritics Tristar II was used to analyze
the surface area and porosity of epoxy particles and porous epoxy. The sample was prepared
in 0.5g. Epoxy particles and porous epoxy were degassing at 200C for 24 hours. The test
was performed at temperature of 77K. The principle of BET is by physical adsorption of
vapour or gas onto the solid surface.

30

3.3.2.2 Density and total pore volume

The relative density and total pore volume of the epoxy particles and porous epoxy
was determined using Helium (He) pycnometer (Micromeritics Ltd, AccuPyc II 1340). It
measure the pore volume using gas displacement method as helium molecules fill the pores
while the solid phase displaces the gas. The AccuPyc II 1340 pynometer provides high
speed, high precision volume measurement and density calculations on a wide variety of
powders, solids and slurries volume from 0.01 to 2000cm3.
Initially, the sample was prepared in weight and then placed into the pycnometer
compartment of known volume. After that, analyses were started with few keystrokes, data
were collected, calculations were performed according to ASTM D 6226 and results
displayed.
Bulk density is determined based on the equation as shown in Eq. 3.1.

b=

wx
wx
=
v b v s + v cp + v op

Where

specimen,

(3.1)

is the bulk density,

vs

wx

is specimen weight,

vb

is solid material volume that without any pore,

closed pores and v op

is bulk volume of the

v cp

is total volume of

is the total volume of open pores [95].

3.3.2.3 Morphology
Epoxy particles and porous epoxy were observed and analyzed by using Dino-Lite
digital microscope (AM5216ZT) at different magnification with Dinocapture 2.0 software.
Microstructure and cross section of epoxy particles and porous epoxy were observed and
analyze using Scanning Electron microscope (SEM) model JSM-6460 LA operating at an
accelerating voltage of 10kV. The epoxy particles and porous epoxy were coated with thin
31

layer of gold in argon atmosphere using sputter coater (Polaron-SC7620) for 90s prior for
observation.
The pores size of porous epoxy and the diameter of epoxy particles on SEM and
optical micrographs were measured using Image J as a image analysis tool. Image J was
used to measure the mean diameters of particles and pores with more than 100 droplets
were included. Besides, the number of distribution of pores and particles can also be
calculated [2].
3.3.2.4 Mechanical Properties
Universal testing machine (UTM) Instron 5560 was used to perform compression
test based on ASTM D 1621 to determine the behaviour of porous epoxy under crushing
loads with 50kN. The porous epoxy prepared was cut into square shape with dimension
50mm x 50mm x 25mm. The test specimen was compressed with cross head speed of 5
mm/min at 253C. After testing and analysis, compressive strength, modulus and
deformation were obtained.

32

Epoxy

Polyamide

Stir at 300 rpm for 3 min

Distilled water

Stir at 1000 rpm for 2 min

Homogenization in 80C water bath

Emulsion viscosity

O/W or W/O emulsion

Gel time
Morphology Characterization
(Optical)

In PP mold

Cure at 80C : 24 hours

Post cure at 110C : 2 hours

Figure 3.1: Flow chart of preparation and characterization of epoxy particles and porous
epoxy.
Epoxy Particles or Porous Epoxy
Morphology
Characterization
Surface area and porosity
CHAPTER
4
(SEM and optical)
PRELIMINARY WORK
Compression test
Density and total pore volume
ASTM 1621

4.1.

Objectives

33

i. To investigate the effect of curing condition on morphology of epoxy particles and

porous epoxy.
ii. To compare polyamide and polyamine in preparation of epoxy particles and porous
epoxy

4.2.

Experimental
4.2.1

Materials

D.E.R 331 Epoxy resin, Polyamide A 062 and Polyamine (Crystal clear epoxy
hardener grade 1618) supplied by DOW Chemical Company.

4.2.2

Methodology

Epoxy and polyamide were pre-mixed homogeneously using an overhead stirrer at

300 rpm for 3 minutes. After that, the epoxy mixture was added into distilled water and
emulsified using an ULTRA-TURRAX homogenizer (IKA) at a speed of 5,000 rpm for 3
minutes under ambient temperature. The resultant emulsion was casted into a
polypropylene (PP) mould. The emulsion morphology was observed using optical
microscope. Then, the casted emulsion was allowed to cure at 80C for 24 hours and post
cure at 110C for 2 hours in an oven and also to vaporize all the distilled water. The process
was repeated with different types of hardener and curing condition.

4.2.3

Testing and Characterization

4.2.3.1 Morphology
The microstructure of epoxy emulsions, epoxy particles and porous epoxy were
visualized using a Dino-Lite digital microscope (AM5216ZT) at different magnification.
The background of the images were adjusted for a white balance and filtered for noise.

34

Photographs of the images were taken using Dinocapture 2.0 software. Image J was used to
measure the mean droplets diameters with more than 100 droplets were included.

4.3.

Results and Discussion

Table 4.1 showed the recipe that used to produce epoxy particle and porous epoxy.
For the formulation 1E:9W, it was expected to get spherical epoxy particles since epoxy
resin is minor component and water is the major component. The water is the continuous
phase that surround the epoxy droplets. Figure 4.1 and 4.2 shows the emulsion and cured
epoxy produced with formulation 9W:1E. From Figure 4.1 (a) it showed that the droplets
dispersed was inhomogeneous due to large difference in droplets size range. The optical
micrograph showed the smallest droplets had diameter of 0.062 mm whereas the largest
diameter of epoxy droplets was 0.642 mm. Besides, it can be seen that there was
flocculation occurs in the epoxy emulsion and air trapped inside the emulsion therefore
three phase exists which include water, epoxy and gas phases. During the homogenization
process carried out, it generates high speed of stirring that can draw the air into the
emulsion and create bubbles. The flocculation of the droplets is a result of instability
emulsion. The epoxy droplets is in constant Brownian motion and this caused the collision
happen between the epoxy droplets. After collide, the droplets can either be in a distant to
each other or floc. As time passed, the gravity forces can cause flocculation take places.
Table 4.1 Recipe of epoxy emulsion.
No. Epoxy/Water Epoxy/Polyamide

1
2
3

Epoxy

Polyamide

Epoxy

Distilled

Ratio

Ratio

(g)

(g)

mixture

water (ml)

1E:9W
1E:9W
9E:W

10E:6PA
10E:5Polyamine
10E:6PA

20.175
22.260
181.575

12.105
11.130
108.945

(ml)
30
30
270

270
270
30

35

Figure 4.1 (b) showed flocculation of droplets since the epoxy droplets had increase
in size. During curing process at room temperature, the epoxy droplets and water molecules
were mobilize in the aqueous phase due to constant Brownian motion and the droplets come
together to each other very close. When the mobile epoxy slide over each other and collide,
the interfacial film that encapsulated the individual droplets broken therefore the droplets
combine to form a single larger droplets which cause coalescence. From Figure 4.1 (c), it
can be seen that the porosity formed from the spherical particles epoxy particle with the
water is very less after it was fully cured. There were little voids left by water after
evaporation. While from the physical appearance shown by Figure 4.2 the white colour
epoxy formed is the particle but it is coalescence and seem almost like continuous phase.
The yellow flakes shaped formed in the upper layer is due to the inhomogeneous of
the emulsion. The top layer of the emulsion is continuous and very thin therefore when post
cure in the oven at 80C, it will easily over cure. This yellowish flakes can be polyamide
since polyamide used is in yellow colour and has the density of 0.96 g/cm 3 which is lower
than water. Hence, the emulsion is separate to 3 layer in which polyamide formed the top
layer, water is in the middle while epoxy is at the bottom. The yellowish flakes will be
characterized under FTIR for further conformation and investigation.

36

Epoxy Droplets

Water
Continuous
Phase

(a)

(b)

(c)
Figure 4.1: Optical micrographs with 9W:1E formulation.
(a) initial condition of emulsion (b) After cured at room temperature for 24 hours
(c) After post cured at 80C in oven for 12 hours

Figure 4.2: Physical appearance of epoxy with formulation 9W:1E after curing process.

37

Figure 4.4 shows the physical appearance of epoxy with formulation 1W:9E. The
formulation with higher volume ratio of epoxy, it is predicted to obtain a porous epoxy. In
this studies, porous epoxy is obtained and it is same as the expectation that made. The
porous epoxy shown is inhomogeneous. When producing emulsion using homogenizer with
5k rpm for 3 minutes, it generates high shear rate which releases heat to the emulsion
system. Besides, the epoxy reaction is an exothermic reaction. The heat absorbed by the
emulsion system can initiate the cross linking reaction of epoxy. The epoxy started to
become more viscous and start to gel obstructs the homogenization. As a result, the
emulsion is non-homogeneous. The porous size also not well distributed.

Figure 4.3: Optical micrographs with 1W:9E formulation.

Figure 4.4: Physical appearance of epoxy with formulation 1W:9E after curing process.

38

Figure 4.5(a) showed the non-uniform of droplets size distribution since the largest
droplets has diameter of 0.042 mm while the smallest diameter was 0.011 mm. The
formation of droplets were also less. The micrograph of the white powdery piece solid
piece consist of porous structure as shown in Figure 4.5 (b) and (c). The porous structure is
formed due to the evaporation of water and left voids there. It is the open cell structure as
the porous is connected with each other. The porosity obtained is more than the Figure 4.1
(c). The yellowish flakes shaped epoxy is obtained as the previous case. In this case, the
emulsion also non-homogeneous as it is separate into 3 layers. From Figure 4.6, the
yellowish flake shaped and the white powdery piece solid piece is obtained.

(a)

(b)

(c)
Figure 4.5: Optical micrographs with 9W:1E formulation (cured at 80C).
(a) initial condition of emulsion (b) After cured at 80C for 24 hours (bottom side)
(c) After cured at 80C for 24 hours (upper side)

39

(a)

(b)

(c)
Figure 4.6: Physical appearance of epoxy after curing process.
(a) The bottom side of epoxy obtained (b) The upper side of epoxy obtained
(c) The result obtained after curing process
Figure 4.7 showed the epoxy emulsion produced by using polyamine as
hardener. It was found that emulsion system show phase separation. Polyamine could
not generate emulsifiability like polyamide does. The emulsifiability characteristic is
due to their own structures. Polyamine which has the linear chain arrangement can lead
to closely packing of the dispersed droplets and therefore it tend to form more
coalescence and hence phase separation. In the other hands, polyamide has more
branched structure and this structure hindered the droplets from coming together to

40

each other. In the other words, it distance the droplets and prevent the coalescence
therefore stabilize the emulsion system

(a)

(b)

Figure 4.7: Images of emulsion with 9W:1E using polyamine

(a) Top view (b) Side view
4.4.

Conclusion
From the result obtained, polyamide is more suitable to use as curing agent in this
research due to it emulsifying chracteristics. Therefore, emulsion instability is minimized.
Room temperature curing caused more coalescence than curing at higher temperature.
Curing at higher temperature also obtained more porous epoxy. The porous epoxy need to
characterized by SEM to check whether epoxy particles is obtained or not. The yellow
flakes shaped epoxy also need to characterized to investigate the problem that encountered.

4.5.

Expectation
The formulation with 9W:1E is expect to get a porous sample with spherical
particles. But in this case, it does not meet the expectation since the emulsion is unstable.
The stability of emulsion is influenced by temperature, time and homogenization speed.
When the emulsion is cured at room temperature, the emulsion stability is fully dependent
on time. For 9W:1E formulation, there is high volume of water which will interrupt the
curing reaction. The longer the curing time, the epoxy droplets have high tendency to
coalesce since it is mobilize in the emulsion system and more time for collision between
each others. Therefore it has higher possibility to break the interfacial film which
encapsulated the droplets. While for the emulsion cured at high temperature in oven, the
41

droplets also gain more energy and the collision between them is more vigorous therefore
cause coalescence. Both curing condition also can also lead to instability emulsion.
Formulation with high water volume is expected to get a more porous sample.
The hardener used to cure the epoxy are polyamide and polyamine. In the emulsion
system carried out, emulsifier and stabilizer is not used. Polyamide is more suitable for
emulsion since it has the emulsifying characteristic.
4.6.

Next Plan
From the studies, it is decided to used polyamide as the curing agent and the curing
condition is set to 80C. For the next laboratory progress, it is plan to carry out the
homogenization at 80C water bath and tend to reduce the duration of homogenization from
3mins to 2mins. This is because the homogenizer agitate at high shear rate which generate
the heat that are non-desirable. The heat generated will cause instability of emulsion. Before
homogenization is carried out, the epoxy mixture and distilled water is pre-stirred for a
more homogeneous mixture and it would not generate the unwanted heat.

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